CN116023151A - Silicon nitride powder manufacturing process - Google Patents
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- CN116023151A CN116023151A CN202310086448.9A CN202310086448A CN116023151A CN 116023151 A CN116023151 A CN 116023151A CN 202310086448 A CN202310086448 A CN 202310086448A CN 116023151 A CN116023151 A CN 116023151A
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- 239000000843 powder Substances 0.000 title claims abstract description 82
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 64
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 23
- 238000005121 nitriding Methods 0.000 claims abstract description 89
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 56
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000011856 silicon-based particle Substances 0.000 claims abstract description 19
- 229910052786 argon Inorganic materials 0.000 claims abstract description 18
- 239000001257 hydrogen Substances 0.000 claims abstract description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000003068 static effect Effects 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001238 wet grinding Methods 0.000 claims abstract description 8
- 239000011148 porous material Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910021419 crystalline silicon Inorganic materials 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 238000004321 preservation Methods 0.000 claims abstract description 5
- 238000003825 pressing Methods 0.000 claims abstract description 5
- 238000012216 screening Methods 0.000 claims abstract description 5
- 210000001161 mammalian embryo Anatomy 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 238000007885 magnetic separation Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000012795 verification Methods 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000010574 gas phase reaction Methods 0.000 description 3
- 239000011863 silicon-based powder Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- YXTPWUNVHCYOSP-UHFFFAOYSA-N bis($l^{2}-silanylidene)molybdenum Chemical compound [Si]=[Mo]=[Si] YXTPWUNVHCYOSP-UHFFFAOYSA-N 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021343 molybdenum disilicide Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention provides a silicon nitride powder manufacturing process, which relates to the technical field of silicon nitride and comprises the following steps: step one: wet grinding the primary crystalline silicon blocks in a ball mill, and using alcohol as a grinding medium to obtain slurry; step two: drying the slurry to obtain powder, and screening the powder; step three: carrying out static pressure treatment on the powder, and pressing the powder into a blank; step four: putting the blank into a nitriding furnace for pre-nitriding; in the nitriding treatment process, pre-nitriding is firstly carried out, then nitriding is carried out at 1250 ℃ for heat preservation, nitrogen, hydrogen and argon are matched, until interweaved silicon nitride monocrystal grains are generated on the surfaces of silicon particles, the pores are filled, nitriding is carried out at 1350-1400 ℃, the silicon nitride of the originally formed network structure continues to develop, grow and compact, and through verification, the prepared silicon nitride powder product has small volume density and high porosity, reduces the strength, and is beneficial to preparing products with complex shapes.
Description
Technical Field
The invention relates to the technical field of silicon nitride, in particular to a silicon nitride powder manufacturing process.
Background
Silicon nitride (Si) 3 N 4 ) Has a series of advantages of high hardness, high strength, wear resistance, high temperature resistance, small thermal expansion coefficient, large heat conductivity coefficient, good thermal shock resistance, low density and the like, has extremely wide application prospect in the fields of ceramic engines, machining, microelectronics, space science, nuclear power engineering and the like, and related products such asSilicon nitride ceramic tool tools, silicon nitride ceramic bearings, automobile engine valves, automobile booster turbines, heaters, various wear-resistant, high-temperature-resistant and corrosion-resistant parts and the like are widely applied to the fields of aviation, electronics, chemical industry, automobiles and the like, and along with the continuous development of silicon nitride ceramic toughening technology and preparation technology, the application of silicon nitride ceramics is continuously expanded, so that the demand for high-performance silicon nitride powder is also increased;
the preparation method of the silicon nitride powder is numerous, and the most widely used methods at present are (1) a direct silicon powder nitriding method; (2) thermal decomposition; (3) carbothermic nitridation; (4) high temperature gas phase reaction process; (5) laser gas phase reaction process; (6) a plasma gas phase reaction process; (7) sol-gel process; (8) self-propagating method. The silicon powder direct nitriding temperature control technology is that a certain amount of energy is provided for a high exothermic chemical reaction system through the outside to induce the chemical exothermic reaction to locally occur, and then the reaction spontaneously expands forward by utilizing the heat released by the reaction until all reactants are converted into products; si3N4 ceramics are widely used in the aspects of ceramic blades, bearings, wire-drawing dies, rollers and the like because of the excellent performances of high strength, high hardness, wear resistance, chemical corrosion resistance and the like; the silicon powder direct nitriding method temperature control technology has the advantages of low production cost, large production scale, higher product quality and the like, and is a synthetic method with great potential and wide prospect in the production of silicon nitride powder; however, in the application of silicon nitride, some products with complex shapes are often required to be prepared, but the silicon nitride prepared in the prior art has higher hardness, and the redundant materials of the silicon nitride ball blank are difficult to remove by adopting the processing mode of the steel ball blank, so that the difficulty is increased for manufacturing the products with complex shapes, and therefore, the invention provides a silicon nitride powder manufacturing process to solve the problems in the prior art.
Disclosure of Invention
In order to solve the problems, the invention provides a silicon nitride powder manufacturing process, and the volume density of the silicon nitride powder product prepared by the silicon nitride powder manufacturing process is 1.827g/cm 3 The porosity is high, the strength is reduced, and the preparation of products with complex shapes is facilitated.
In order to achieve the purpose of the invention, the invention is realized by the following technical scheme: a process for preparing silicon nitride powder comprises the following steps:
step one: wet grinding the primary crystalline silicon blocks in a ball mill, and using alcohol as a grinding medium to obtain slurry;
step two: drying the slurry to obtain powder, and screening the powder;
step three: carrying out static pressure treatment on the powder, and pressing the powder into a blank;
step four: putting the embryo body into a nitriding furnace for pre-nitriding, controlling the temperature to be 900-1100 ℃, introducing mixed gas of 95% nitrogen and 5% hydrogen into the nitriding furnace, and nitriding for 11.5 hours;
step five: nitriding and preserving heat at 1250 ℃ until interweaved silicon nitride monocrystal grains are generated on the surfaces of the silicon particles, and filling the pores among the silicon particles in the blank;
step six: nitriding at 1350-1400 ℃ to enable the originally formed silicon nitride with a network structure to continue to develop, grow and compact through the reaction of nitrogen and solid silicon particles;
step seven: detecting the appearance of the embryo body, and stopping nitriding after the appearance of the embryo body meets the preparation standard;
step eight: and (3) putting the blank into a pulverizer, and performing ball milling and acid washing treatment to obtain silicon nitride powder.
The further improvement is that: in the first step, wet grinding is carried out in a ball mill to obtain slurry with the particle size of 0.05mm-0.07 mm.
The further improvement is that: in the second step, the slurry is dried at the temperature of 80-100 ℃ to remove the water in the slurry, so as to obtain the powder.
The further improvement is that: in the second step, powder is screened, and powder with the particle size larger than 0.1mm is removed.
The further improvement is that: in the third step, before static pressure treatment, a magnetic separation roller is used for adsorbing metal impurities in the powder, and in the third step, the powder is put into a vacuum press, and is pressed into a blank body by adopting 100-120Mpa pressure for static pressure.
The further improvement is that: in the fourth step, during pre-nitriding, the nitriding furnace is selected as a backing plate in the nitriding furnace, the nitriding degree is controlled to 9%, and in the fourth step, argon is introduced when the temperature is raised to 1000 ℃, and the nitrogen amount is 2/3 of the nitrogen amount.
The further improvement is that: in the fifth step, nitriding is performed for 4 hours at 1250 ℃, and nitrogen, hydrogen and argon are introduced in the nitriding process.
The further improvement is that: in the sixth step, nitriding is performed for 8 hours at 1350 ℃, the nitriding degree is controlled to be 51%, nitriding is continuously performed for 28 hours at 1350 ℃, the nitriding degree is controlled to be 61%, nitriding is performed for 2 hours at 1450 ℃, and in the sixth step, when the temperature is raised to 1350 ℃, argon is stopped after heat preservation is performed for 3 hours, and the nitrogen and hydrogen atmosphere is recovered.
The further improvement is that: in the seventh step, in the detection process, it is mainly detected whether the network structure formed on the blank body meets the required standard, the standard and the workpiece to be prepared need to be specifically set, and in the seventh step, after the nitridation is stopped, the blank body is cooled at normal temperature.
The further improvement is that: in the eighth step, the green body balls are ground into powder with the particle size of 1-3um, then cleaning liquid with the pH value smaller than 2 is used for carrying out acid cleaning on the powder after ball milling, and the silicon nitride powder is obtained after acid cleaning and drying.
The beneficial effects of the invention are as follows:
1. in the nitriding treatment process, the pre-nitriding is firstly carried out to 9 percent of nitriding degree, then the nitriding is carried out at 1250 ℃ for heat preservation, and nitrogen, hydrogen and argon are matched for introducing until the surface of silicon particles generates interweaved silicon nitride monocrystal grains, the gaps among silicon particles in a blank are filled, and then the nitriding is carried out at 1350-1400 ℃ to ensure that the originally formed silicon nitride with a network structure continuously grows, grows and is compact, and through verification, the volume density of the silicon nitride powder product prepared by the invention is 1.827g/cm 3 The porosity is high, the strength is reduced, and the preparation of products with complex shapes is facilitated.
2. The invention ball-mills the embryo into powder, then uses the cleaning liquid with the PH value less than 2 to acid-wash the ball-milled powder, and can obtain silicon nitride powder with the purity up to 99.99 percent after verification, thereby improving the product quality.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The present invention will be further described in detail with reference to the following examples, which are only for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
Example 1
According to fig. 1, this embodiment provides a process for manufacturing silicon nitride powder, which includes the following steps:
step one: wet grinding the primary crystalline silicon blocks in a ball mill, and using alcohol as a grinding medium to obtain slurry;
step two: drying the slurry to obtain powder, and screening the powder;
step three: carrying out static pressure treatment on the powder, and pressing the powder into a blank;
step four: putting the embryo body into a nitriding furnace for pre-nitriding, controlling the temperature to be 900-1100 ℃, introducing mixed gas of 95% nitrogen and 5% hydrogen into the nitriding furnace, and nitriding for 11.5 hours;
step five: nitriding and preserving heat at 1250 ℃ until interweaved silicon nitride monocrystal grains are generated on the surfaces of the silicon particles, and filling the pores among the silicon particles in the blank;
step six: nitriding at 1350-1400 ℃ to enable the originally formed silicon nitride with a network structure to continue to develop, grow and compact through the reaction of nitrogen and solid silicon particles;
step seven: detecting the appearance of the embryo body, and stopping nitriding after the appearance of the embryo body meets the preparation standard;
step eight: and (3) putting the blank into a pulverizer, and performing ball milling and acid washing treatment to obtain silicon nitride powder.
In the nitriding treatment process, the method comprises the steps of pre-nitriding, nitriding to 9 percent, nitriding at 1250 ℃ and preserving heat, and introducing nitrogen, hydrogen and argon until the surface of the silicon particle generates interwoven silicon nitrideMonocrystalline grains are filled in the pores among silicon particles in the blank, and then nitriding is carried out at 1350-1400 ℃ to ensure that the originally formed silicon nitride with a network structure continues to develop, grow and compact, and through verification, the volume density of the silicon nitride powder product prepared by the invention is 1.827g/cm 3 The porosity is high, the strength is reduced, and the preparation of products with complex shapes is facilitated.
Example two
According to fig. 1, this embodiment provides a process for manufacturing silicon nitride powder, which includes the following steps:
wet milling the primary crystalline silicon block in a ball mill, using alcohol as a milling medium, and wet milling in the ball mill to obtain slurry with the particle size of 0.05-0.07 mm;
drying the slurry at 80-100deg.C, removing water to obtain powder, and screening to remove powder with particle diameter greater than 0.1 mm; the particle size of the powder is controlled, so that the qualification rate of the raw materials is kept, and the subsequent processing quality is optimized;
before static pressure treatment, firstly adsorbing metal impurities in the powder by using a magnetic separation roller, then carrying out static pressure treatment on the powder, putting the powder into a vacuum press, carrying out static pressure by adopting the pressure of 100-120Mpa, and pressing into a blank; the metal impurities in the powder are adsorbed by the magnetic separation roller, so that the influence on the subsequent nitriding quality is avoided;
putting the embryo into a nitriding furnace for pre-nitriding, selecting the nitriding furnace as a backing plate in the nitriding furnace, controlling the temperature to be 900-1100 ℃, introducing mixed gas of 95% nitrogen and 5% hydrogen into the nitriding furnace, nitriding for 11.5 hours, and controlling the nitriding degree to be 9%; when the temperature is raised to 1000 ℃, argon is introduced, and the nitrogen amount is 2/3 of that of the argon; the nitriding furnace can use a molybdenum wire electric furnace or a molybdenum disilicide rod electric furnace, the hearth is tightly sealed to ensure vacuumizing and use safety, silicon and nitrogen begin to react at about 970-1000 ℃, and the reaction rate is accelerated along with the temperature rise, but if the temperature rises quickly to exceed the melting point of silicon, the blank can collapse due to the melting of silicon. Therefore, nitriding is carried out in advance at a temperature far below the melting point, the nitriding furnace is in a mixed atmosphere of 95% of nitrogen and 5% of hydrogen, and the liner plate in the furnace is silicon nitride;
nitriding at 1250 ℃ for 4 hours, and introducing nitrogen, hydrogen and argon in the nitriding process until interweaved silicon nitride monocrystal grains are generated on the surfaces of silicon particles, so that the pores among the silicon particles in the blank are filled;
nitriding at 1350-1400 ℃ to enable the originally formed silicon nitride with a network structure to continue to develop, grow and compact through the reaction of nitrogen and solid silicon particles; nitriding for 8 hours at 1350 ℃, controlling the nitriding degree to be 51%, continuously nitriding for 28 hours at 1350 ℃, controlling the nitriding degree to be 61%, nitriding for 2 hours at 1450 ℃, completely nitriding, keeping the temperature for 3 hours when the temperature is raised to 1350 ℃, stopping introducing argon, and recovering the nitrogen and hydrogen atmosphere; since nitrogen reacts with silicon as an exothermic reaction, the initial reaction of nitriding is rapid, and a large amount of heat is generated to cause local temperature to exceed the melting point of silicon and melt and exude. When the temperature is raised to 1000 ℃, argon (accounting for 2/3 of the nitrogen) is started to be introduced, the argon is stopped after the temperature is kept for a period of time to 1350 ℃, and the atmosphere of 95% nitrogen and 5% hydrogen is restored, so that the argon can be used for buffering the excessive reaction speed. Before completion, argon is stopped, otherwise excessive reaction occurs.
3Si+2N 2 (g)＝Si 3 N 4 (1)
3Si+4NH 3 (g)＝Si 3 N 4 +6H 2 (g) (2)
Detecting the appearance of the embryo body, and stopping nitriding after the appearance of the embryo body meets the preparation standard; in the detection process, mainly detecting whether a network structure formed on the blank body meets the required standard, wherein the standard and a workpiece to be prepared need to be specifically set, and after stopping nitriding, cooling the blank body at normal temperature;
and (3) putting the embryo body into a pulverizer, grinding the embryo body into powder with the particle size of 1-3um, then carrying out acid washing on the powder after ball milling by using a cleaning solution with the pH value less than 2, and drying after acid washing to obtain silicon nitride powder. Through verification, the silicon nitride powder with the purity of up to 99.99 percent can be obtained, and the product quality is improved.
Verification example:
therefore, the silicon nitride powder prepared by the invention has small volume density and low strength, and is beneficial to preparing products with complex shapes.
The preparation process of the silicon nitride powder comprises the steps of pre-nitriding at the nitriding degree of 9%, nitriding at 1250 ℃ for heat preservation, and introducing nitrogen, hydrogen and argon until the surfaces of silicon particles generate interweaved silicon nitride monocrystal grains, filling the pores among silicon particles in a blank, nitriding at 1350-1400 ℃ to enable the originally formed silicon nitride with a network structure to continue to develop, grow and compact, and the verification proves that the volume density of the silicon nitride powder product prepared by the preparation process is 1.827g/cm 3 The porosity is high, the strength is reduced, and the preparation of products with complex shapes is facilitated. The green body is ball-milled into powder, and then the ball-milled powder is pickled by using a cleaning solution with the pH value less than 2, and the silicon nitride powder with the purity of 99.99 percent can be obtained through verification, so that the product quality is improved.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The silicon nitride powder manufacturing process is characterized by comprising the following steps of:
step one: wet grinding the primary crystalline silicon blocks in a ball mill, and using alcohol as a grinding medium to obtain slurry;
step two: drying the slurry to obtain powder, and screening the powder;
step three: carrying out static pressure treatment on the powder, and pressing the powder into a blank;
step four: putting the embryo body into a nitriding furnace for pre-nitriding, controlling the temperature to be 900-1100 ℃, introducing mixed gas of 95% nitrogen and 5% hydrogen into the nitriding furnace, and nitriding for 11.5 hours;
step five: nitriding and preserving heat at 1250 ℃ until interweaved silicon nitride monocrystal grains are generated on the surfaces of the silicon particles, and filling the pores among the silicon particles in the blank;
step six: nitriding at 1350-1400 ℃ to enable the originally formed silicon nitride with a network structure to continue to develop, grow and compact through the reaction of nitrogen and solid silicon particles;
step seven: detecting the appearance of the embryo body, and stopping nitriding after the appearance of the embryo body meets the preparation standard;
step eight: and (3) putting the blank into a pulverizer, and performing ball milling and acid washing treatment to obtain silicon nitride powder.
2. A process for preparing silicon nitride powder as defined in claim 1, wherein: in the first step, wet grinding is carried out in a ball mill to obtain slurry with the particle size of 0.05mm-0.07 mm.
3. A process for preparing silicon nitride powder as defined in claim 2, wherein: in the second step, the slurry is dried at the temperature of 80-100 ℃ to remove the water in the slurry, so as to obtain the powder.
4. A process for producing silicon nitride powder according to claim 3, wherein: in the second step, powder is screened, and powder with the particle size larger than 0.1mm is removed.
5. A process for preparing silicon nitride powder as defined in claim 4, wherein: in the third step, before static pressure treatment, a magnetic separation roller is used for adsorbing metal impurities in the powder, and in the third step, the powder is put into a vacuum press, and is pressed into a blank body by adopting 100-120Mpa pressure for static pressure.
6. A process for preparing silicon nitride powder as defined in claim 5, wherein: in the fourth step, during pre-nitriding, the nitriding furnace is selected as a backing plate in the nitriding furnace, the nitriding degree is controlled to 9%, and in the fourth step, argon is introduced when the temperature is raised to 1000 ℃, and the nitrogen amount is 2/3 of the nitrogen amount.
7. A process for preparing silicon nitride powder as defined in claim 6, wherein: in the fifth step, nitriding is performed for 4 hours at 1250 ℃, and nitrogen, hydrogen and argon are introduced in the nitriding process.
8. A process for preparing silicon nitride powder as defined in claim 7, wherein: in the sixth step, nitriding is performed for 8 hours at 1350 ℃, the nitriding degree is controlled to be 51%, nitriding is continuously performed for 28 hours at 1350 ℃, the nitriding degree is controlled to be 61%, nitriding is performed for 2 hours at 1450 ℃, and in the sixth step, when the temperature is raised to 1350 ℃, argon is stopped after heat preservation is performed for 3 hours, and the nitrogen and hydrogen atmosphere is recovered.
9. A process for preparing silicon nitride powder as defined in claim 8, wherein: in the seventh step, in the detection process, it is mainly detected whether the network structure formed on the blank body meets the required standard, the standard and the workpiece to be prepared need to be specifically set, and in the seventh step, after the nitridation is stopped, the blank body is cooled at normal temperature.
10. A process for preparing silicon nitride powder as defined in claim 9, wherein: in the eighth step, the green body balls are ground into powder with the particle size of 1-3um, then cleaning liquid with the pH value smaller than 2 is used for carrying out acid cleaning on the powder after ball milling, and the silicon nitride powder is obtained after acid cleaning and drying.
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| CN102030536A (en) * | 2010-11-18 | 2011-04-27 | 宁波华标特瓷采油设备有限公司 | Method for preparing silicon nitride powder with low energy consumption and cost |
| US20120141349A1 (en) * | 2008-12-13 | 2012-06-07 | Alzchem Trostberg Gmbh | Method for producing high-purity silicon nitride |
| CN103332662A (en) * | 2013-07-11 | 2013-10-02 | 上海大学 | Method for preparing alpha phase and beta phase silicon nitride powder by improved direct nitriding method |
| CN108529576A (en) * | 2017-03-03 | 2018-09-14 | 苏州协鑫能源技术发展有限公司 | Silicon nitride and preparation method thereof |
| CN111792937A (en) * | 2020-07-14 | 2020-10-20 | 中材高新氮化物陶瓷有限公司 | Preparation method of silicon nitride powder |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120141349A1 (en) * | 2008-12-13 | 2012-06-07 | Alzchem Trostberg Gmbh | Method for producing high-purity silicon nitride |
| CN102030536A (en) * | 2010-11-18 | 2011-04-27 | 宁波华标特瓷采油设备有限公司 | Method for preparing silicon nitride powder with low energy consumption and cost |
| CN103332662A (en) * | 2013-07-11 | 2013-10-02 | 上海大学 | Method for preparing alpha phase and beta phase silicon nitride powder by improved direct nitriding method |
| CN108529576A (en) * | 2017-03-03 | 2018-09-14 | 苏州协鑫能源技术发展有限公司 | Silicon nitride and preparation method thereof |
| CN111792937A (en) * | 2020-07-14 | 2020-10-20 | 中材高新氮化物陶瓷有限公司 | Preparation method of silicon nitride powder |
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